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NAME MATRIC NO PROGRAMME : Nur Azhani bt Ab Aziz : 156306 : Bac Sc( Hons)- Industrial Chemistry
PARTNER NAME MATRIC NO PROGRAMME
: Izwaharyanie bt Ibrahim : 156342 : Bac Sc( Hons)- Industrial Chemistry
: Preparation Of Double Salt and Complex Salt
NO.OF EXPERIMENT : 4
: 19 September 2011
EXPERIMENT 4 TITLE : PREPARATION OF DOUBLE SALT AND COMPLEX SALT OBJECTIVES : After carrying out the experiment. the complex part can be either cation or anion. Epsom sals are also an example of a double salt. we are able to : 1. 2.6H2O. A well-known double salt is alum containing two cations (sodium and aluminium) and a sulfate anion. Then it form a deep purplish blue solution when dissolve in excess ammonia. Sometimes it also can be both anion and cation. For example. Synthesise double salt and complex salt using wet chemistry method. In order to prepare a complex salt. and does not lose its identity with such addition compound. Ca3[Co(Cl)6]2 the complex part behaves as an anion and [Co(NH3)6]Cl3 the complex part behaves as a cation. Complex salt is formed when an addition compound is dissolve in water or organic solvent and it does not dissociate. Double salt has two different cations in their crystal lattice in a definite proportion and they commonly form large crystal more readily than the single salt that made them up. Alums are double sulphates of a monovalent cation and a trivalent cation containing 24 water of crystallization. does not give its constituent ions. They form when more than one salt is dissolved in a liquid and when together they crystallize in a regular pattern. . INTRODUCTION : A double salt is a salt that crystallizes as a single substances but ionizes as two distinct salts when dissolved. A complex salt is the salt of one or more complex ions. as a carnallite KMgCl3 . Characterise and compare the physical and chemical properties between the prepared salts. H2O. Double salts contain more than one cation or anion. which need not be the same as that of either component. The color is due to the complex ion Cu (NH3)4 and the sulphate of this ion is easily obtained in solid form as the hydrated Cu (NH3)4 SO4. They have their own crystal forms. Other example are potassium sodium tartrate and bromlite. a light blue precipitate of cupric hydroxide is first formed when ammonia is added to a solution of a cupric salt.
Cu (NH3) SO4. CuSO4 (NH4)2 SO4 . H2O 6.25g CuSO4. 10 ml of ethyl alcohol was added slowly The solution was allowed to stand for an hour It was cooled inside the ice bath .5H2O + 3.96 g of 0.03 mol of CuSO4.6H2O 7.METHODOLOGY : (A) Preparation of double salt .49 g of 0.5H2O + 6ml water + 10ml concentrated ammonia Then.03 mol (NH4)2 SO4 15 ml hot water The solution was left aside to let it cool slowly mix and dissolve The crystal was filtered by using Buchner funnel It was let to dried on filter paper The crystal was weight and recorded (B) Preparation of complex salt.
followed by alcohol then ether.The crystal was filtered by using Buchner funnel The crystal was wash with equal amount volume of alcohol and concentrated ammonia. The crystal was let to dried The crystal was weight and recorded .
56 Frequency (cm-1) Complex salt 3231. H2O Double salt Weight of filter paper Weight of yield + filter paper Weight of yield Comparison between properties of double salt and complex salt Properties Colour Solubility in alcohol Solubility in water Physical state IR Type of bond N-H S-O Cu-S Cu-N UV There is a peak occur at 807. 6H2O and complex salt Cu(NH3)4 SO4.32 1617. CuSO4 (NH4).RESULTS : For double salt. Frequency (cm-1) Double salt 3124.56 Double salt Light blue Not soluble Not soluble Solid Complex salt Dark blue Soluble Slightly soluble Solid Complex salt .64 1401.82 1099. However for complex salt.39 nm with 0.30 1402.502 absorption for double salt.62 1112. there was no peak that can be determined.40 1630.
5H2O = 0. 5H2O (aq) + (NH4)2 SO4 (aq) + H2O From the equation above : CuSO4 (NH4)2 SO4.44 + 32.14 g∕mol :: Mass of (NH4)2 SO4 used in experiment = 0.008) 16.58 = 7.008) ] + 32.4874 g No. 5H2O = 63. of mole of (NH4)2 SO4 = 0.CALCULATION : ( A ) Preparation of double salt.9642 g The equation of reaction : CuSO4.58 g ∕mol :: Mass of CuSO4.03 mole Relative molecular mass CuSO4.00 ] = 249.03 x 249.064 + 4(16. of mole of CuSO4. CuSO4(NH4)3 SO4.00) + 5[ 2(1.0067 + 4(1. 5H2O used in the experiment = 0.14 =3. 6H2O (s) .03 x 132. 6H2O Mass determination of double salt No.064 + 4(16.00) = 132.03 mole Relative molecular mass of (NH4)2 SO4 = 2 [ 14.
8165 g∕mol Theoretical mass of CuSO4 (NH4)2 SO4.0)+6[2(1..03 x 397.064 + 4(16.0067+ 3(1. 6H2O :: 0.6H2O = 63. 6H2O = 0. 5H2O (aq) + 4NH3 (aq) Cu(NH3)4 SO4. 5H2O ≡ 0.008) + 16.00) + 2(1.008)] + 32.8165 = 11. ( B ) Preparation of complex salt. of mole of Cu(NH3)4 SO4.0] = 397. 6H2O Formula mass of CuSO4 (NH4)2.7428 g∕mol The reaction equation : CuSO4.064+4(16.0)+2[14.03mole of CuSO4.9345) x 100% =…………………….∕11. Cu(NH3)4 SO4. The percentage error = (11.54 + 4 [14.1mole of CuSO4.H2O No.54 32.9345) x 100% The percentage yield = (experimental yield ∕ theoretical yield) x 100% = (………∕11.9345 g The mass of double salt obtained from the experiment =……………….008)]+32. H2O = 0 Relative molecular mass of Cu(NH3)SO4. H2O (s) + 4H2O .00 =245. H2O = 63.5H2O ≡ 1mole of CuSO4. (NH4)2 SO4.008) + 16.9345-……….03mole of CuSO4(NH4)2 SO4.0067+3(1.064+4(16.
.g Mass of complex salt obtained from the experiment =…….g The percentage error = …….H2O ::………………. Theoretical mass of Cu(NH3)4 SO4. . The percentage yield = ( experimental yield∕ theoretical yield ) x 100% =…….From the equation : 1mole of CuSO4. 5H2O ≡ 1mole of Cu(NH3)4 SO4.H2O =……… =……….
g. There might be a salt that is not well filtered. The color of the solution turn color due to the formation of Cu2+ ions. H2O. In part A of the experiment.DISCUSSION : In this experiment. While the mass that we obtained for complex salt. the mass of double salt.%. There are also some problem when we need to take the weight of the salts. which is less than the theoretical value. Then the solution was left inside the ice bath for an hour. in UV-VIS spectroscopy. CuSO4(NH4)2 SO4.39nm with 0. From this experiment. While carrying out this experiment there might be some errors occurred that may effects the percentage of yield to be less than the theoretical value. Thus the yield percentage that is obtained is…. The crystal that formed was in dark blue color. the cooling down process need to be done slowly. It will formed a dark blue solution due to the formation of Cu(NH3)4 2+ complex ions. 6H2O and Cu(NH3)4 SO4..502 absorption. for double salt there is no peak occur at 807. Furthermore. H2O is….…g. when we prepared CuSO4(NH4)2 SO4. 6H2O is …….%. In order for us to get a perfect and good crystal sample. which is less than the theoretical value……. The color of the solution turn to light blue crystal when the cooling process was done. for the complex salt. there is no peak that can be determined.While in part B of the experiment. . the salt might not well wash using the ammonia and ether. we might not do it the right way. the complex salt Cu(NH3)4 SO4.g. The reading of the analytical balance was not stable maybe due to the impurities from the previous experiment that was left inside it. Let the solution cool down for a few minutes before we can get the result. This steps is important to make sure that the complex ions will form completely. The double salt is much more soluble than the complex salt because of the formation of complex ions Cu(NH3)4 2+ in complex salt. 6H2O is formed when copper sulphate pentahydrate and ammonium sulphate was dissolved in hot water for a several minutes.H2O was produced when the cupric salt is dissolved in excess ammonia. For example when we filtered the salt.g. Thus the yield percentage that is obtained is…. Cu(NH3)4 SO4 . the double salt CuSO4(NH4)2 SO4. Besides that. The reason that we used ice bath in this experiment is to help the process of recrystallization occur a lot faster than the usual. While for complex salt.we can observe the behaviour between double salt and complex salt and also the difference in their constitution.
Silver (Ag). 6H2O ]. the difference constitution is [ Cu (NH3 )4 ²+ ] is a complex ion and for double salt. NH4+. 5H2O + 4NH3 + H2O Cu(NH3)4 SO4 . So. (2) Name three other metallic cations that form complex ions with ammonia. H2O formed. Thus. cobalt ammonium sulphate [ CoSO4 (NH4)2 SO4. 5H2O salt. PRECAUTION STEPS : 1. make sure all the salts are transferred perfectly into the Buchner funnel. Some of the complex ion is reverse to the CuSO4 . . Cu²+. Nickel (Ni). 5H2O was added to the water. H2O + 5H2O. When doing the filteration steps. and Cobalt (Co) (3) When the complex salt is dissolve in water. Therefore. when CuSO4. What is this precipitate. Rinse all the apparatus completely with distilled water before we used. 3.QUESTIONS : (1) Name three double salt that are important in industry or in laboratory practice. make sure that the crystal are dried completely in the oven. 2KCl . The complex salts must be rinsed properly with ammonia and ether. H2O is a complex salt with the elements of ion [ Cu (NH3)4 ²] and [ SO4. It is a reversible reaction. CuSO4 . NH4+ is a cation. ammonium nickel sulphate [ (NH4)2 SO4 NiSO4 . 2H2O ]. H+ and OH-. 2. 6H2O is a double salt with the elements of ion Cu². complex ion of Cu ( NH3)4 SO4 . a slight precipitate is appear. and why is it formed ? CuSO4 . 6H2O ]. SO4². Before we do the weighing process.] while CuSO4 ( NH4 )2 SO4 . The three double salts are calcium copper chloride [ CuCl2 . 4. (4) What is the difference in constitution between tetrammine cupric sulphate and cupric ammonium sulfate? Cu (NH3)4 SO4 . 5H2O salt is the precipitate.
Double salt is soluble in water. The mass of complex salt. CuSO4 (NH4) SO4. The mass of double salt.. 6H2O obtained is…g.% 2. Cu(NH3)4 SO4 . While the percentage of yield is…% 3. The crystal of double salt is light blue colour.CONCLUSION 1. While the percentage of yield is. while complex salt is slightly soluble in water REFERENCES . whereas the crystal of complex salt is dark blue colour.H2O is …g. 4.
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